CN105833810A - A preparing method of a composite polyelectrolyte microcapsule - Google Patents
A preparing method of a composite polyelectrolyte microcapsule Download PDFInfo
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- CN105833810A CN105833810A CN201610220344.2A CN201610220344A CN105833810A CN 105833810 A CN105833810 A CN 105833810A CN 201610220344 A CN201610220344 A CN 201610220344A CN 105833810 A CN105833810 A CN 105833810A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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Abstract
The invention relates to a preparing method of a composite polyelectrolyte microcapsule and belongs to the field of composite materials. The method includes a step of preparing a CaCO3 template with negative charges, a step of cladding sodium polystyrenesulfonate (PSS) and poly(allylamine) hydrochloride (PAH) layer by layer on the CaCO3 template through functions of electrostatic, and a step of removing CaCO3 template particles. The prepared microcapsule has a capability of embedding a plurality of medicines, has good release response performance, and has a wide development space in the life medical field.
Description
Technical field
The present invention relates to the preparation method of a kind of composite polyelectrolyte microcapsule, belong to field of compound material.
Background technology
Different phase in application disease treatment typically requires specific drug release degree, and therefore sustained release rate and slow-release period are weighing apparatuses
The important indicator of amount drug microcapsule application effect.Intellectual drug induction system generally requires outside stimulus just can show slow-releasing
Can, therefore environmental response type composite polyelectrolyte microcapsule is the ideal material being applied to medicine conveying.According to filmogen not
With, microcapsule is when outside stimulus occurs, under pH value, salt, photo-thermal or metabolite effect, and its size, shape and infiltration
Property also presents different or reversible changes.Due to the nano-scale that microcapsule is special, dissimilar Nano medication microcapsule
Construct and microcapsule carrier is the emphasis of current drug microcapsule aspect research to the mechanism of action of drug molecule.
In the world, existing considerable part scientific research institution investigated the composite polyelectrolyte microcapsule with environment-responsive.This
The NEW TYPE OF COMPOSITE polyelectrolyte multiplayer microcapsule that patent relates to has higher drug loading because having high specific surface area, therefore exists
Field of drug delivery has great application prospect.
Summary of the invention
The present invention improves in said method thinking, and preparation has the composite polyelectrolyte microcapsule of certain response performance；Make
Use certain density Na2CO3Solution and Ca (NO3)2·4H2O solution prepares CaCO3Template, uses autonomous packing technique layer by layer,
And use polyallylamine hydrochloride (PAH) solution and kayexalate salt (PSS) solution alternate group to be contained in template CaCO3
On, finally with certain density sodium ethylene diamine tetracetate solution enucleation, it is achieved that the system to the microcapsule with embedding multi-medicament
Standby.
For achieving the above object, the technical solution used in the present invention is as follows:
The preparation method of a kind of composite polyelectrolyte microcapsule, comprises the following steps:
(1) prepared by template: by Na2CO3Solution and the Ca (NO containing kayexalate salt (PSS)3)2·4H2O solution mixes,
Stand, to solution, layering occurs, supernatant is removed and i.e. obtains the CaCO with negative charge3Microgranule；
(2) cladding of wall material: by CaCO3Fine-particle powder is dispersed in polyallylamine hydrochloride (PAH) solution, in water-bath
In agitator after vibration, centrifuge washing, ground floor is completed；Then the micro-of a layer polypropylene amine hydrochlorate (PAH) will be assembled with
Grain powder is dispersed in kayexalate salt (PSS) solution, and under the same terms, water-bath vibration, centrifuge washing, be so one
Double-deck assembling.Repeat above operation, prepare difference and assemble (PAH/PSS) of the number of pliesnComposite micro-capsule；
(3) template is removed: the CaCO that will process through cladding3Microgranule is distributed in sodium ethylene diamine tetracetate (EDTA) solution, water
After bath vibration, take out centrifugal, remove supernatant, clean with deionized water, repeat above operating process, thoroughly to remove CaCO3
Template particles, i.e. obtains composite hollow microcapsule；
Na described in above-mentioned steps (1)2CO3The concentration of solution is 0.1-1mol/L.
Ca (NO described in above-mentioned steps (1)3)2·4H2The concentration of O solution is 0.1-1mol/L.
Ca (NO described in above-mentioned steps (1)3)2·4H2The concentration of the PSS in O solution is 1-8mg/mL.
Described in above-mentioned steps (1), time of repose is 15-40min.
CaCO described in above-mentioned steps (2)3The concentration of Nanoparticle Solution is 1-5g/mL.
Described in above-mentioned steps (2), the concentration of polyallylamine hydrochloride (PAH) solution is 0.5-5g/L.
Described in above-mentioned steps (2), the number of times of centrifuge washing is 1-5 time.
Described in above-mentioned steps (2), the concentration of kayexalate salt (PSS) solution is 0.5-5g/L.
Described in above-mentioned steps (3), the concentration of sodium ethylene diamine tetracetate (EDTA) solution is 0.1-0.5mol/L, the consumption of solution
For 15-50mL.
CaCO described in above-mentioned steps (3)3Microgranule time of water-bath vibration in sodium ethylene diamine tetracetate solution is 15-45min.
The superiority of the present invention:
In textile printing and dyeing field, this composite polyelectrolyte microcapsule can be used for cladding and the controllable release dyeing course of dyestuff, can carry
The effective rate of utilization of high dyestuff, and owing to the cladding effect of microcapsule, beneficially dyeing and finishing processing industry contaminating the process of waste water, right
In environmental conservation, there is actively impact；And microcapsule can be coated with some have health care or the medicine for the treatment of function, arrangement to knitting
Thing surface, can develop good Biomedical Textiles.Additionally, in field of medicine release, relative to normal structure, tumor
Tissue vasculogenic epithelial cells arrangement around is irregular so that can pass through tumor by the microcapsule within Normal tissue vascular
Tissue blood vessel arrives near cancerous cell, therefore has certain targeting for cancerous cell, and when microcapsule by cancerous cell endocytosis it
After, the synergism of bulk effect and medicament slow release effect can accelerate inducing cell apoptotic process, effectively reduces the multiple medicines of cancerous cell
Drug resistance, for the solution that the structure offer of the associating diagnosis and treatment drug platform of cancer is good.Therefore composite polyelectrolyte microcapsule
In the transport of functional composite material targeting and controllable sustained-release field, there is splendid application prospect.
Accompanying drawing explanation
Fig. 1 is the result photo of the embodiment of the present invention 1；
Fig. 2 is the result photo of the embodiment of the present invention 2；
Fig. 3 is the result photo of the embodiment of the present invention 3
Detailed description of the invention
The present invention is described below in conjunction with the accompanying drawings with specific embodiment.Unless stated otherwise, technological means used in the present invention
It is method known in those skilled in the art.It addition, embodiment is interpreted as illustrative, and the unrestricted present invention
Scope, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this
On the premise of invention spirit and scope, the various changes or the change that carry out the material component in these embodiments and consumption also belong to
In protection scope of the present invention.
Embodiment 1:
By Na2CO3Solution and the Ca (NO being mixed with polyelectrolyte PSS3)2Solution mixes, and prepares the CaCO doped with PSS3
Template particles.Observe putting into doped with the calcium carbonate template that molecular weight is 70K under TM-1000 ultramicroscope, through surveying
Examination obtains CaCO3The MIcrosope image of template particles, as shown in Figure 1 photo, doped with PSS calcium carbonate template granularity relatively
Uniformly, concordance is preferable.
Embodiment 2:
Being dissolved in a certain amount of water by trace stratiform microcapsule pressed powder, sonic oscillation makes it be uniformly dispersed, after dilution
Microcapsule solution liquid-transfering gun drips on microscope slide (1-2 drips), and microscope slide is placed on super depth of field three-dimensional microscope by covered
(VHX-1000) observe under.Obtain photo as shown in Figure 2, be assembled with (PSS/PAH)2Microcapsule have clearly
Hollow structure, fully shows that the template particles that multilayer film is coated with fully is removed by EDTA, and separates from capsule.
Embodiment 3:
By rhodamine B (RhB) solution soaking 24h of dried microcapsule 1g/ml, the microcapsule after soaking is cleaned 4 times.
In order to study the release to rhodamine B (RhB) dyestuff of the PAH/PSS composite micro-capsule.Under conditions of 37 DEG C, will be embedded with
(PAH/PSS) of RhB2Microcapsule, discharges respectively in the buffer of pH=5.8 and 7.4, at set intervals, takes portion
Subrelease tapping utilizes UV-1200 ultraviolet spectrophotometer to carry out absorbance test, calculates RhB in the release liquid under different time
Concentration, obtains Concentration-time release profiles.Obtain photo as shown in Figure 3.
Claims (11)
1. a preparation method for composite polyelectrolyte microcapsule, comprises the following steps:
(1) prepared by template: by Na2CO3Solution and the Ca (NO containing kayexalate salt (PSS)3)2·4H2O solution mixes, and stands and layering occurs to solution, is removed by supernatant and i.e. obtain the CaCO with negative charge3Microgranule；
(2) cladding of wall material: by CaCO3Fine-particle powder is dispersed in polyallylamine hydrochloride (PAH) solution, and in water bath chader after vibration, centrifuge washing, ground floor is completed；Then being dispersed in kayexalate salt (PSS) solution by the fine-particle powder being assembled with a layer polypropylene amine hydrochlorate (PAH), water-bath vibration under the same terms, centrifuge washing, is so double-deck assembling.Repeat above operation, prepare difference and assemble (PAH/PSS) of the number of pliesnComposite micro-capsule；
(3) template is removed: the CaCO that will process through cladding3Microgranule is distributed in sodium ethylene diamine tetracetate (EDTA) solution, after water-bath vibration, takes out centrifugal, removes supernatant, clean with deionized water, repeat above operating process, thoroughly to remove CaCO3Template particles, i.e. obtains composite hollow microcapsule.
The preparation method of a kind of composite polyelectrolyte microcapsule, it is characterised in that the Na described in above-mentioned steps (1)2CO3The concentration of solution is 0.1-1mol/L.
The preparation method of a kind of composite polyelectrolyte microcapsule, it is characterised in that the Ca (NO described in above-mentioned steps (1)3)2·4H2The concentration of O solution is 0.1-1mol/L.
The preparation method of a kind of composite polyelectrolyte microcapsule, it is characterised in that Ca (NO described in above-mentioned steps (1)3)2·4H2The concentration of the PSS in O solution is 1-8mg/mL.
The preparation method of a kind of composite polyelectrolyte microcapsule, it is characterised in that described in above-mentioned steps (1), time of repose is 15-40min.
The preparation method of a kind of composite polyelectrolyte microcapsule, it is characterised in that the CaCO described in above-mentioned steps (2)3The concentration of Nanoparticle Solution is 1-5g/mL.
The preparation method of a kind of composite polyelectrolyte microcapsule, it is characterised in that described in above-mentioned steps (2), the concentration of polyallylamine hydrochloride (PAH) solution is 0.5-5g/L.
The preparation method of a kind of composite polyelectrolyte microcapsule, it is characterised in that described in above-mentioned steps (2), the number of times of centrifuge washing is 1-5 time.
The preparation method of a kind of composite polyelectrolyte microcapsule, it is characterised in that described in above-mentioned steps (2), the concentration of kayexalate salt (PSS) solution is 0.5-5g/L.
A kind of preparation method of composite polyelectrolyte microcapsule, it is characterized in that, described in above-mentioned steps (3), the concentration of sodium ethylene diamine tetracetate (EDTA) solution is 0.1-0.5mol/L, and the consumption of solution is 15-50mL.
The preparation method of 11. a kind of composite polyelectrolyte microcapsules, it is characterised in that CaCO described in above-mentioned steps (3)3Microgranule time of water-bath vibration in sodium ethylene diamine tetracetate solution is 15-45min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108486879A (en) * | 2018-06-08 | 2018-09-04 | 天津工业大学 | A kind of preparation method of natural polysaccharide LBL self-assembly microcapsules |
| CN110629556A (en) * | 2019-10-09 | 2019-12-31 | 天津工业大学 | Method for finishing pure cotton fabric by using traditional Chinese medicine rhizoma atractylodis-loaded microcapsules |
| CN111613457A (en) * | 2020-04-28 | 2020-09-01 | 赵灶生 | Preparation method of high-strength self-repairing polyelectrolyte composite material |
| CN115785774A (en) * | 2023-01-29 | 2023-03-14 | 天津市科莱博瑞科技有限公司 | Method for preparing polythiophene/polystyrene sulfonic acid/nano silver composite conductive dispersion liquid by utilizing microcapsule technology |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108486879A (en) * | 2018-06-08 | 2018-09-04 | 天津工业大学 | A kind of preparation method of natural polysaccharide LBL self-assembly microcapsules |
| CN110629556A (en) * | 2019-10-09 | 2019-12-31 | 天津工业大学 | Method for finishing pure cotton fabric by using traditional Chinese medicine rhizoma atractylodis-loaded microcapsules |
| CN111613457A (en) * | 2020-04-28 | 2020-09-01 | 赵灶生 | Preparation method of high-strength self-repairing polyelectrolyte composite material |
| CN115785774A (en) * | 2023-01-29 | 2023-03-14 | 天津市科莱博瑞科技有限公司 | Method for preparing polythiophene/polystyrene sulfonic acid/nano silver composite conductive dispersion liquid by utilizing microcapsule technology |
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Application publication date: 20160810 |